CN116206942A - Ionization source structure of multiple light sources for mass spectrum field - Google Patents

Ionization source structure of multiple light sources for mass spectrum field Download PDF

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Publication number
CN116206942A
CN116206942A CN202310173434.0A CN202310173434A CN116206942A CN 116206942 A CN116206942 A CN 116206942A CN 202310173434 A CN202310173434 A CN 202310173434A CN 116206942 A CN116206942 A CN 116206942A
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CN
China
Prior art keywords
ion
electrode
inlet
transmission
ultraviolet light
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CN202310173434.0A
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Chinese (zh)
Inventor
韩文奎
车欣欣
陈伟章
李庆运
王磊
王东鉴
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Shenzhen Berui Biotechnology Co ltd
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Shenzhen Berui Biotechnology Co ltd
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Priority to CN202310173434.0A priority Critical patent/CN116206942A/en
Publication of CN116206942A publication Critical patent/CN116206942A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • H01J49/16Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
    • H01J49/161Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission using photoionisation, e.g. by laser
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/26Mass spectrometers or separator tubes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/10Nuclear fusion reactors

Abstract

The invention discloses an ionization source structure of multiple light sources for mass spectrum field, comprising: an inlet insulating gasket, an inlet ion electrode, a transmission ion electrode and an ion extraction electrode are arranged in the vacuum insulating ring from top to bottom along the axial direction; the inlet ion electrode, the ion transmission electrode and the ion extraction electrode are all of a structure of a central through hole, and the central through holes are coaxial and are arranged in parallel at intervals; the first sample inlet is arranged at the upper end of the vacuum insulation ring, and is coaxially arranged with the inlet ion electrode, the ion transmission electrode and the ion extraction electrode; the vacuum ultraviolet light sources are distributed and arranged around the central axis of the first sample inlet. The distribution area of vacuum ultraviolet light in the ionization source cavity is increased, and the ionization rate and the sensitivity of an ion mobility spectrogram are improved.

Description

Ionization source structure of multiple light sources for mass spectrum field
Technical Field
The invention relates to the field of ionization source structures of mass spectrometers, in particular to an ionization source structure with multiple light sources for the field of mass spectrometry.
Background
The atmospheric pressure photoelectric ionization technology is the most common ionization technology used in a time-of-flight mass spectrometer, and vacuum ultraviolet light can enable organic molecules with ionization energy lower than photon energy to generate single photon ionization, mainly generate molecular ions, almost have no fragment ions, has simple spectrogram, can perform quick qualitative and quantitative analysis according to molecular weight and signal intensity, is easy to analyze, is the most common ionization technology used in the mass spectrometry field, and is widely applied to detection fields of volatile organic pollutants, explosives, drugs, chemical toxicants and the like.
A time-of-flight mass spectrometer is a mass spectrometer that creates a mass spectrum by ions arriving at a detector at different times at different mass-to-charge ratios within a distance vacuum field-free region. The ion source has the advantages of simple structure, high ion flow rate, unrestricted mass range and the like, sample molecules fly to the rear field-free drift tube under the action of an electric field after being ionized in the ionization source cavity, the larger the mass of the ions is, the slower the flying speed is, the longer the time for the ions to reach the rear receiver is, and according to the principle, the ions with different masses can be separated by distinguishing the time for the ions to reach the rear. However, existing time-of-flight mass spectrometers remain deficient in that the use of a single vacuum ultraviolet light source does not provide different fragment information and suitable compounds for different ionization sources.
In order to ensure good ion transmission efficiency, the ionization region inner diameter of the time-of-flight mass spectrometer is usually set to 8-24mm, and the photoionization source ion mobility spectrometry generally uses commercial VUV lamps, and the beam diameter of the output vacuum ultraviolet light of the commercial VUV lamps is smaller and is only about 8 mm. This results in the presence of vacuum ultraviolet light within the ionization source chamber only in the columnar region immediately adjacent to the source axis under conventional single vacuum ultraviolet light source conditions, and the absence of vacuum ultraviolet light in the radial region slightly off axis within the ionization region. Meanwhile, because the concentration distribution of mixed sample molecules in the ionization region is also uneven, only a part of samples in the ionization region are ionized by vacuum ultraviolet light to form product ions, the ionization rate of the sample molecules is low, and the detection sensitivity of an ion mobility spectrogram is low.
Accordingly, there is a need for an ionization source structure for multiple light sources in the mass spectrometry field that addresses one or more of the above problems.
Disclosure of Invention
The present invention provides an ionization source structure with multiple light sources for mass spectrometry. The invention adopts the technical proposal for solving the problems that: an ionization source structure for multiple light sources in the mass spectrometry field, comprising: an inlet insulating gasket, an inlet ion electrode, a transmission ion electrode and an ion extraction electrode are arranged in the vacuum insulating ring from top to bottom along the axial direction, and an ion transmission cavity is formed;
the ion transmission electrodes are at least provided with one, and when the number of the ion transmission electrodes is greater than one, the ion transmission electrodes are mutually separated by an insulating sealing gasket;
the inlet ion electrode, the ion transmission electrode and the ion extraction electrode are all of a structure of a central through hole, and the central through holes are coaxial and are arranged in parallel at intervals;
the first sample inlet is arranged at the upper end of the vacuum insulation ring, and is coaxially arranged with the inlet ion electrode, the ion transmission electrode and the ion extraction electrode;
the vacuum ultraviolet light sources are distributed around the central axis of the first sample inlet, and emit light beams towards the inner side direction of the ion transmission cavity.
In some embodiments, the vacuum ultraviolet light source is arranged in a conical surrounding manner along the central axis of the first sample inlet, the emission end of the vacuum ultraviolet light source is close to the central axis of the first sample inlet, and the other end of the vacuum ultraviolet light source is far away from the central axis of the first sample inlet;
the included angle between the vacuum ultraviolet light source and the axis of the first sample inlet is 10-80 degrees.
In some embodiments, further comprising: the output section of the second sample inlet is perpendicular to the first sample inlet.
In some embodiments, the inlet ion electrode, the ion transmitting electrode and the ion extraction electrode are sequentially loaded with different voltages in order of absolute value of the voltages from high to low, and an ion extraction electric field of 0-500V/cm is formed in the axial direction.
In some embodiments, an upper section of the central through hole of the inlet ion electrode is provided with a thin-walled flange extending in the axial direction of the central through hole of the inlet ion electrode.
In some embodiments, the ion-transporting electrodes are in a ring structure, and when the number of the ion-transporting electrodes is greater than one, a plurality of ion-transporting electrodes are arranged in a coaxial and parallel manner;
the ion transmission electrode is provided with an air hole and a light transmission hole, and the air hole and the light transmission hole are used for allowing sample molecules and vacuum ultraviolet light to pass through;
when the number of the ion transmission electrodes is larger than one, a plurality of ion transmission electrodes are sequentially loaded with different voltages from top to bottom according to the absolute value of the voltages.
In some embodiments, when the number of the ion transmission electrodes is greater than one, the diameters of the central through holes of all the ion transmission electrodes are equal, or the diameters of the central through holes of the ion transmission electrodes gradually decrease from top to bottom, and the air pressure of the ion transmission cavity is 10pa-1000pa.
In some embodiments, the diameter of the central through hole of the entrance ion electrode is 1-20mm, the diameter of the central through hole of the transport ion electrode is 1-20mm, and the diameter of the central through hole of the ion extraction electrode is 0.1-5mm.
In some embodiments, when the number of ion-transporting electrodes is greater than one, the distance between adjacent ion-transporting electrodes is 0.5-25mm.
In some embodiments, the number of the vacuum ultraviolet light sources is 2-8, and a plurality of the vacuum ultraviolet light sources are mutually independent, and are any one or more of a gas discharge lamp, an ultraviolet light emitting diode, a synchrotron radiation light source and a laser light source.
The beneficial value obtained by the invention is as follows: according to the invention, the vacuum insulating ring, the inlet insulating gasket, the inlet ion electrode, the ion transmission electrode, the ion extraction electrode and the vacuum ultraviolet light source form an ionization source structure of a plurality of light sources for the mass spectrum field, so that the distribution area of vacuum ultraviolet light in the ionization source cavity is increased by a simpler structure, and compared with the existing structure, more vacuum ultraviolet light distribution areas can be obtained by using a small amount of vacuum ultraviolet light sources, and the ionization rate of neutral sample molecules in the ionization area is improved; the number of ions entering the mass spectrometer from the ionization sample is increased by forming the central through holes of the plurality of electrodes into a funnel shape, so that the number of ions detected by the rear-end mass spectrometer is more, and the sensitivity of an ion mobility spectrogram is further improved. The practical value of the invention is greatly improved.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a comparative graph of the implementation effect of the present invention;
FIG. 3 is a diagram showing the effects of a simion simulation example of the present invention;
fig. 4 is a table of parameter settings for a simion simulation example effect diagram of the present invention.
[ reference numerals ]
1 first sample inlet
2 vacuum ultraviolet light source
Insulating spacer for inlet
4 inlet ion electrode
5. Vacuum insulation ring
6 ion extraction electrode
7 & lt- & gt transmitting ion electrode
8 second sample inlet
9. The ion beam was simulated.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention briefly described above will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The invention may be embodied in many other forms than described herein without departing from the spirit or scope of the invention as defined in the following claims.
As shown in fig. 1, the present invention discloses an ionization source structure of multiple light sources for mass spectrometry, which comprises: a vacuum insulating ring 5, in which an inlet insulating gasket 3, an inlet ion electrode 4, a transmission ion electrode 7 and an ion extraction electrode 6 are arranged from top to bottom along the axial direction in the vacuum insulating ring 5, and an ion transmission cavity is formed;
at least one transmission ion electrode 7 is arranged, and when the number of the transmission ion electrodes 7 is more than one, the transmission ion electrodes 7 are separated from each other through an insulating sealing gasket;
the inlet ion electrode 4, the transmission ion electrode 7 and the ion extraction electrode 6 are all in a structure of central through holes, and the central through holes are coaxial and are arranged in parallel at intervals;
the first sample inlet 1 is arranged at the upper end of the vacuum insulation ring 5, and the first sample inlet 1, the inlet ion electrode 4, the transmission ion electrode 7 and the ion extraction electrode 6 are arranged coaxially;
the vacuum ultraviolet light sources 2 are distributed and arranged around the central axis of the first sample inlet 1, and the vacuum ultraviolet light sources 2 emit light beams towards the inner side direction of the ion transmission cavity.
Specifically, as shown in fig. 1, the vacuum ultraviolet light source 2 is arranged in a conical shape around the central axis of the first sample inlet 1, the emission end of the vacuum ultraviolet light source 2 is close to the central axis of the first sample inlet 1, and the other end of the vacuum ultraviolet light source 2 is far away from the central axis of the first sample inlet 1;
the included angle between the vacuum ultraviolet light source 2 and the axis of the first sample inlet 1 is between 10 and 80 degrees, that is, the included angle between the emitted light beam of the vacuum ultraviolet light source 2 and the axis of the first sample inlet 1 can be controlled between 10 and 80 degrees, so as to increase the distribution area of vacuum ultraviolet light.
Further comprises: the second sample inlet 8, the output section of the second sample inlet 8 is perpendicular to the first sample inlet 1, and the first sample inlet and the second sample inlet can be used for sampling different samples.
Specifically, as shown in fig. 1, in the implementation, the inlet ion electrode 4, the transmission ion electrode 7 and the ion extraction electrode 6 are sequentially loaded with different voltages in order of higher absolute value of voltage, and an ion extraction electric field of 0-500V/cm is formed in the axial direction.
As shown in connection with fig. 1, in practice, the upper section of the central through hole of the inlet ion electrode 4 may be provided with a thin-walled flange extending in the axial direction of the central through hole of the inlet ion electrode 4. The voltage at the thin-wall flange has a repulsive interaction with ions entering the ionization source cavity, and is equivalent to an ion repulsive electrode, and the voltage at the inner wall of the lower side of the thin-wall flange is used as an ion transmission electrode.
And the ion transmission electrodes 7 are in a ring structure, and when the number of the ion transmission electrodes 7 is more than one, a plurality of ion transmission electrodes 7 are coaxially and parallelly arranged;
the ion transmission electrode 7 is provided with air holes and light holes, and the air holes and the light holes are used for allowing sample molecules and vacuum ultraviolet light to pass through;
when the number of the ion transmission electrodes 7 is larger than one, a plurality of ion transmission electrodes 7 are sequentially loaded with different voltages from top to bottom according to the absolute value of the voltages;
when the number of the ion transmission electrodes 7 is greater than one, the diameters of the central through holes of all the ion transmission electrodes 7 are equal, or the diameters of the central through holes of the ion transmission electrodes 7 are gradually reduced from top to bottom (the cross section forms a funnel shape), and the air pressure of the ion transmission cavity is 10pa-1000pa.
In particular, in practice, the parameter settings for each component of the present invention may be: the diameter of the central through hole of the inlet ion electrode 4 is 1-20mm, the diameter of the central through hole of the ion transmission electrode 7 is 1-20mm, and the diameter of the central through hole of the ion extraction electrode 6 is 0.1-5mm;
when the number of the ion transfer electrodes 7 is greater than one, the distance between adjacent ion transfer electrodes 7 is 0.5 to 25mm.
In the implementation of the present invention, the vacuum uv light sources 2 are generally independent of each other, so that the number of the vacuum uv light sources 2 can be controlled according to the measured sample or the detection requirement, so as to form vacuum uv light distribution areas with different shapes or sizes, and the number of the vacuum uv light sources 2 can be 2-8. The vacuum ultraviolet light source 2 is any one or more of a gas discharge lamp, an ultraviolet light emitting diode, a synchrotron radiation light source and a laser light source, and the multiple light sources are matched to meet the requirements.
The inlet insulating gasket 3 and the insulating sealing gasket are made of PEEK. The invention can be used in quadrupole mass spectrometry, time-of-flight mass spectrometry, ion trap mass spectrometry, fourier transform cyclotron resonance mass spectrometry and magnetic mass spectrometry detection systems.
In implementation, sample molecules enter an ionization source cavity through a capillary (the first sample inlet and the second sample inlet), are ionized under the action of ultraviolet light to form gas-phase ions, and the gas-phase ions transmit the sample ions to the ion extraction electrode 6 under the action of electric field force generated by the inlet ion electrode 4 and the transmission ion electrode 7 and then enter a mass spectrometer through the ion extraction electrode 6 to finish mass spectrum detection analysis. Compared with the traditional time-of-flight mass spectrometer, the invention has the advantages that the multi-lamp sharing is realized to improve the beam distribution area, and the number of the vacuum ultraviolet light sources 2 used is smaller than that of the traditional structure; the above-mentioned distribution arrangement mode of the vacuum ultraviolet light source 2 can realize that ultraviolet light fills the ionization source cavity channel with less quantity, increase the probability of contacting sample molecules with ultraviolet light, and then increase the ionization quantity of sample molecules and improve the ionization efficiency of ions; on the axial section, each electrode forms a funnel-shaped channel, so that more reactant ions are focused and led in to pass through the ion extraction electrode 6 at the back, more ions participating in subsequent reactions are caused, and the reaction efficiency is improved.
By increasing the ionization base number in the ionization cavity, improving the ion reaction efficiency and leading more ions through the ion extraction electrode 6, the number of ions detected by the rear-end mass spectrum is increased, and the high-sensitivity detection of the low-concentration characteristic organic matters is realized.
The implementation structure is that the ionization source structure of the invention detects 1ppm standard gas under the fixed conditions of a vacuum ultraviolet Kr lamp of 10.6eV and sampling time of 60s, the number of the vacuum ultraviolet light sources 2 is changed, and the signal intensity comparison diagram obtained by a rear-end mass spectrometer is shown as figure 2. As can be seen from fig. 2, single lamp ionization: double lamp ionization: the signal intensity of three lamp ionization substantially corresponds to 1:2:3, the ionization source structure of the invention can enhance and improve the instrument signal by increasing the number of lamps, and has excellent enhancement effect, thereby effectively improving the detection sensitivity.
Referring to fig. 3 and 4, the present invention is simulated on the simion (electrostatic lens analysis simulation software) under the initial ion setting parameters shown in the table of fig. 4, fig. 3 is a simulation effect diagram, and as can be seen from the simulation ion beam 9 in fig. 3, the structure of the present invention has a better ion focusing effect and a higher transmission efficiency for ion transmission.
In summary, the vacuum insulation ring, the inlet insulation gasket, the inlet ion electrode, the ion transmission electrode, the ion extraction electrode and the vacuum ultraviolet light source form an ionization source structure with multiple light sources for the mass spectrum field, so that the vacuum ultraviolet light distribution area in the ionization source cavity is increased by a simpler structure, and compared with the existing structure, more vacuum ultraviolet light distribution areas can be obtained by using a small amount of vacuum ultraviolet light sources, and the ionization rate of neutral sample molecules in the ionization area is improved; the number of ions entering the mass spectrometer from the ionization sample is increased by forming the central through holes of the plurality of electrodes into a funnel shape, so that the number of ions detected by the rear-end mass spectrometer is more, and the sensitivity of an ion mobility spectrogram is further improved.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. Wherein the terms "first position" and "second position" are two different positions.
The foregoing examples are merely representative of one or more embodiments of the present invention and are described in more detail and are not to be construed as limiting the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of the invention should be assessed as that of the appended claims.

Claims (10)

1. An ionization source structure of a multiple light sources for mass spectrometry, comprising: an inlet insulating gasket, an inlet ion electrode, a transmission ion electrode and an ion extraction electrode are arranged in the vacuum insulating ring from top to bottom along the axial direction, and an ion transmission cavity is formed;
the ion transmission electrodes are at least provided with one, and when the number of the ion transmission electrodes is greater than one, the ion transmission electrodes are mutually separated by an insulating sealing gasket;
the inlet ion electrode, the ion transmission electrode and the ion extraction electrode are all of a structure of a central through hole, and the central through holes are coaxial and are arranged in parallel at intervals;
the first sample inlet is arranged at the upper end of the vacuum insulation ring, and is coaxially arranged with the inlet ion electrode, the ion transmission electrode and the ion extraction electrode;
the vacuum ultraviolet light sources are distributed around the central axis of the first sample inlet, and emit light beams towards the inner side direction of the ion transmission cavity.
2. The ionization source structure of multiple light sources for mass spectrometry according to claim 1, wherein the vacuum ultraviolet light source is arranged in a conical shape along the central axis of the first sample inlet, the emission end of the vacuum ultraviolet light source is close to the central axis of the first sample inlet, and the other end of the vacuum ultraviolet light source is far away from the central axis of the first sample inlet;
the included angle between the vacuum ultraviolet light source and the axis of the first sample inlet is 10-80 degrees.
3. The ionization source structure of multiple light sources for mass spectrometry according to claim 1, further comprising: the output section of the second sample inlet is perpendicular to the first sample inlet.
4. The ionization source structure of a multiple light source for mass spectrometry according to claim 1, wherein the entrance ion electrode, the transmission ion electrode, and the ion extraction electrode are sequentially loaded with different voltages in order of higher absolute value of voltage, and an ion extraction electric field of 0-500V/cm is formed in the axial direction.
5. The ionization source structure of a multiple light source for mass spectrometry according to claim 1, wherein an upper section of the center through hole of the inlet ion electrode is provided with a thin-walled flange extending toward an axial direction of the center through hole of the inlet ion electrode.
6. The ionization source structure of multiple light sources for mass spectrometry according to claim 1, wherein the ion-transmitting electrodes are in a ring structure, and when the number of the ion-transmitting electrodes is greater than one, a plurality of the ion-transmitting electrodes are arranged in a coaxial and parallel manner;
the ion transmission electrode is provided with an air hole and a light transmission hole, and the air hole and the light transmission hole are used for allowing sample molecules and vacuum ultraviolet light to pass through;
when the number of the ion transmission electrodes is larger than one, a plurality of ion transmission electrodes are sequentially loaded with different voltages from top to bottom according to the absolute value of the voltages.
7. The ionization source structure of claim 1 or 6, wherein when the number of the ion transmission electrodes is greater than one, the diameters of the central through holes of all the ion transmission electrodes are equal, or the diameters of the central through holes of the ion transmission electrodes are gradually reduced from top to bottom, and the air pressure of the ion transmission cavity is 10pa-1000pa.
8. The ionization source structure of claim 1, wherein the diameter of the central through hole of the entrance ion electrode is 1-20mm, the diameter of the central through hole of the transmission ion electrode is 1-20mm, and the diameter of the central through hole of the ion extraction electrode is 0.1-5mm.
9. The ionization source structure of a multiple light source for mass spectrometry according to claim 1 or 8, wherein when the number of the ion-transporting electrodes is greater than one, the distance between adjacent ion-transporting electrodes is 0.5 to 25mm.
10. The ionization source structure of multiple light sources for mass spectrum field according to claim 1, wherein the number of the vacuum ultraviolet light sources is 2-8, the multiple vacuum ultraviolet light sources are mutually independent, and the vacuum ultraviolet light sources are any one or more of gas discharge lamp, ultraviolet light emitting diode, synchrotron radiation light source and laser light source.
CN202310173434.0A 2023-02-20 2023-02-20 Ionization source structure of multiple light sources for mass spectrum field Pending CN116206942A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117711910A (en) * 2024-02-02 2024-03-15 中国科学院合肥物质科学研究院 Multi-source photoionization source focused by quadrupole ion funnel and sensitivity enhancement method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117711910A (en) * 2024-02-02 2024-03-15 中国科学院合肥物质科学研究院 Multi-source photoionization source focused by quadrupole ion funnel and sensitivity enhancement method

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